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This schematic illustrates what happens in a distillation column. A liquid mixture is fed into the
distillation column. On entering the column, the heated feed is partially vaporized and rises up
the column. However, as it rises, it cools by contacting the descending cooler liquid and partially
condenses so that, while part of vapor continues to flow upward, the condensed portion is
enriched in the less volatile component(s) and flows downward. As the vapor continues to flow
upward, it undergoes partial condensation a number of times and each time becomes richer in the
more volatile component(s).
Group 3
Shrikant Shah
Brandon Farr
Alex Georg
Michael Ogiefo
Mohammed Khatib
Ghassan Alkhateeb
Table of Contents
1. WP&C.....................................................................................................................................2
1. Introduction............................................................................................................................3
2. Theory......................................................................................................................................5
3. Apparatus..............................................................................................................................13
4. Materials and Supplies.........................................................................................................18
5. Procedure..............................................................................................................................19
8. Error Analysis.......................................................................................................................21
9. References.............................................................................................................................22
1. WP&C
What is the purpose of this experiment?
The purpose of this experiment is separate a mixture of a 5% wt methanol-water solution in a binary distillation
column. About 0.1-2 GPM of methanol-water mixture will be introduced into the round bottom flask of the column.
The column will operate at temperatures ranging from 0-100oC. The column will be run and allowed to reach steady
state before samples from the six stages will be obtained and tested with a Refractometer to eventually obtain the
methanol concentration in each stage.
What are the hazards associated with the experiment?
1. Methanol is relatively toxic fluid. It can cause eye, skin and respiratory tract irritation when carelessly
exposed to lab personnel.
2. The electrical wires for the thermocouples are carelessly exposed. If lab personnel were to accidentally touch
them while conducting experiment, they run the risk of an electric shock.
3. The persistent use of fluids like water and methanol could lead to fluid spillage. If lab personnel were to walk
over an affected area, they run the risk of injuries due to a fall.
1. Introduction
Distillation is a physical separation process that uses the differences in volatility between
compounds in a liquid mixture. Binary distillation separates two liquid components from one
another. All fluids possess some degree of volatility that is a measure of their tendency to
vaporize. A higher volatile compound such as methanol will vaporize more quickly when
compared to water under the same atmospheric conditions. Boiling the two components would
also make the difference even more apparent, as the less volatile water would boil at a higher
temperature than the methanol. More importantly, even when two components are mixed
together, the unique physical properties of the individual component still causes the more volatile
compounds at equilibrium. At the boiling point of a mixture, the more volatile component exists
as a greater fraction in the vapor than it will in the liquid. In a methanol-water mixture,
distillation would yield a greater mole fraction of methanol in the vapor than in the liquid.
Condensing the vapor and adding more distillation steps or stages in series is the basis for
continuous distillation. When a continuous system is arranged vertically, the system is defined
as a distillation column. In such a column, falling liquids vaporize at lower stages and rising
vapors condense at higher ones. A heat source at the bottom of the column enables this action,
creating a decreasing temperature gradient up the column. With more distillation steps greater
Distillation columns are widely used for separations in industry, most notably in
petroleum, natural gas, and chemical processing, as well as any other large-scale liquid
volatility. Medicinal herbs can be distilled from plant matter in the pharmaceutical industry.
In this experiment, we will distill a mixture of methanol and water in a column distiller.
The apparatus has six trays that will act as the stages of the continuous distillation. Collection of
the condensate at each of these stages will allow an analysis of the composition at each plate.
The temperature will also be recorded at each stage. Ultimately, decreasing temperatures and
equilibrium data will allow a comparison between experimental results and theoretical trends.
2. Theory
Distillation is the separation, by vaporization, of different components in a mixture
because of the different volatilities that they possess at a given boiling point of the mixture.
When a mixture reaches a specific temperature and pressure a certain amount of the mixture
moves into the vapor phase until the vapor reaches the mixtures vapor pressure. This point is
pressure at a set pressure and temperature in a specific mixture. It is incorrectly assumed that the
components of a mixture will separate based on their boiling points when pure. Rather, the
boiling point of a mixture is based on the total vapor pressure of a mixture, which is a sum of the
vapor pressures of each individual component in the mixture. This is known as Daltons law.
sat
P = (v pa + v pb ) (1)
Where,
sat
P [=] Vapor pressure of mixture [kPa]
v pa
[=] Vapor pressure of component a [kPa]
v pb
[=] Vapor pressure of component b [kPa]
This means that a component will not boil off cleanly meaning it is impossible through
distillation to obtain a pure substance. The vapor created above a mixture is also a mixture of
components. The composition of the vapor is based on the volatility of each of the substances.
Raoults law helps us to determine what the volatility, or K value of a substance. This in turn
v pa x a
y a= (2)
psat
Where:
ya
[=] mole fraction of component a in vapor phase (dimensionless)
v pa
[=] vapor pressure of component a [kPa]
xa
[=] mole fraction of component a in liquid phase (dimensionless)
Not all mixtures obey Raoults law. Some components that have high solubility with each
other form azeotrope. An azeotrope is a mixture that has either a higher or lower boiling point
than the boiling point of any of the pure components. This means that when a mixture reaches an
azeotrope, such as ethanol and water at 95.6 % water, it behaves as a pure substance.
The simplest of all distillation techniques is called flash distillation. Flash distillation occurs
when a mixture at a specific temperature and pressure is allowed to drop in pressure. This
changes the vapor-liquid equilibrium of the mixture and creates a vapor rich in the most volatile
component(s). This is also the crudest form of distillation and does not allow for refinement of
the distillates.
A more complicated form of distillation is batch distillation. Batch distillation uses both a
boiler and a condenser, but only allows one separation, or cut, to be taken from the mixture.
Figure 1: A schematic of a typical continuous distillation tower. A is the kettle that holds the
liquid mixture, B is the Reboiler that adds heat to the mixture, C is the distillation column that
holds the trays or packing, D is the condenser that turns the distillate to a liquid product.
Continuous distillation is the most complicated and most common form. It has a boiler,
condenser and multiple trays or packing which allows the vapor to condense as it moves up the
column and cools. The trays or packing allows for a better separation of the components in the
mixture which in the end gives purer products. It also adds a lot of complexity to the system.
Figure 2: A typical tray in a distillation column. A is the tray itself, B are the holes in the tray
that allow the vapor to pass through the tray, C and D are the tubes that allow liquid to pass from
one tray to another. As the vapor moves up the column it gets progressively cooler which allows
some of the mixture to condense and further concentrates the vapor with the lightest
component(s).
Figure 3: This shows a simple McCabe-Thiele diagram. The number of steps corresponds to the
number of trays needed for a given mixture.
Determining the size of the tower and the number of trays needed was historically a very
difficult process involving many calculations. The McCabe-Thiele method greatly simplified that
process. The method uses a graphical representation of the material balance equations as
operating lines on a graph of the liquid composition (x-axis) and the vapor composition (y-axis).
The bottom line in Figure 3 is the x-y line. This starts at the origin and ends where x and y both
equal 1.This line would represent a distillation column that operated at total reflux and total boil-
up, meaning that all of the vapor and all of the liquid is recycled back into the system. The next
line added is the vapor liquid equilibrium line for a binary system which is found
experimentally. By moving step-wise between the two lines we can find the number of
theoretical plates needed for a specific separation of a binary mixture and the liquid and vapor
composition at any point in the distillation column. These stage lines can be seen in Figure 3.
Figure 4: McCabe-Thiele diagram with operating lines and feed line added.
In practice, we want to draw a purified product out of the column in the form of either a
distillate (top of the column) or the bottoms product (bottom of the column) or both. This
requires a column that operates at a partial reflux and/or a partial boil-up ratio. This means that
we cannot use the x-y line for such a column. In Figure 4 we see the addition of a line for reflux
ratio (slope L/V) and a line for the boil-up (slope L/V). The boil-up lines slope increases as we
increase the amount of bottoms product that we remove from the system. Subsequently, as we
remove more distillate as product we decrease the slope of the top operating line, which is the
line for the reflux ratio. By changing the amount of liquid re-boiled, which is liquid returned to
the column as a vapor, or by changing the amount of vapor refluxed, returned to the column as a
liquid, we change the number of theoretical plates necessary for a given separation. The q
(quality) line in Figure 4 is the feed line which is the composition of the stream entering the
distillation column. We can see from the diagram in Figure 4 that where that line intersects with
the two operating lines is the feed stage, or the tray at where the incoming stream enters.
LL H h f
q= (3)
F Hh
Where:
q ZF
y= ( q1 ) x + 1q (4)
Where:
L0 L0
y=
D
L0
(1+ )
D
x + 1
( )
D
1+
x
L0 D
D
(5)
Where:
The McCabe-Thiele method is widely used for binary mixtures. When dealing with multi-
component mixtures addition assumptions and calculations are necessary. There are a number of
issues that need to be watched when sizing a continuous distillation column properly. They are:
Foaming- foaming occurs when the gas passing upward causing the liquid to bubble
excessively. While this normally depends on the properties of the liquid, it can also be caused by
Entrainment- Occurs when the vapor velocity is too high due to a column having too
small of a diameter. This causes liquid to be held up at the trays and does not allow proper
Weeping- Occurs when the vapor velocity is too low. When the velocity drops too low,
liquid starts to fall, or weep, through the holes in the plates. This does not allow enough liquid to
get to the re-boiler which means that the entire column needs to be shut down and re-started.
Flooding- This occurs when liquid entrainment become too severe. This causes a large
3. Apparatus
22
24
T8
Figure 5 represents the Binary Distillation apparatus without any of the support beams. The column is
constructed of a round bottom flask (7) which holds a methanol- water solution. This solution is distilled by
applying electrical energy to the heating jacket (24) which heats up the solution causing the volatile liquids and
gases to rise. Total reflux occurs in the system by feeding cooling water (10) into a cooling coil (16) at the top
of the column. Thermocouples (T1-T9) measure the temperatures at various points in the system and output
them onto an electrical temperature monitor (21). Liquid and gaseous samples are taken at ever one of the 6
stages via sample ports (L1-L6 &G1-G6) and tested with a Refractometer to calculate the density and
eventually the composition of the samples.
Table 1: Binary Distillation Apparatus Summary (For Figure 5)
Component No. Apparatus Component Manufacturer Description Notes/Safety
Water Connection for Check for leaks and cracks.
1 ChE Unit Ops Water supplied by lab
Apparatus Clean up spills immediately.
Check for leaks and cracks that
2 Water Supply Valve MCD Used to load water into Storage Tank.
could cause malfunctions.
3 Funnel Na Used to ease filling of solutions Do not overfill
Used to load 5 mol% ethanol solution Check for cracks and overall
4 13 Gallon Feed Tank Nalgene
before filling flask structural integrity.
Only open when filling round bottom Check for leaks and cracks that
5 Feed Supply Valve Nalgene
flask could cause malfunctions.
Valve is labeled to either drain, fill or Check for leaks and cracks that
6 Three way valve Swagelok
prevent loss could cause malfunctions.
Do not heat when empty!!
Ensure flask is cooled before
Used to hold the Methanol-water
7 Round Bottom Flask Na adding any fluid Look for any
solution
leaks or cracks before adding
solution or heat.
Located at different heights along the
Check for cracks and leaks that
8 Valves & Sample Ports Nalgene column to obtain experimental
could cause malfunctions.
samples
Each section at collection point is
pieced together. The top piece Examine entire column for any
9 Glass sections of column Na contains the cooling water tubes and leaks, cracks or anything that
a narrowed opening so that total could fracture structural integrity
reflux can be assumed.
Always open when distillation
Cooling water Connection
10 ChE Unit Ops Cooling water is supplied by lab column is in operation to supply
for Apparatus.
ample cold water.
Always open when distillation
Cold Chicago Used to start flow of cooling water
11 Cooling Water Supply Valve column is in operation to supply
Faucets into system.
ample cold water.
Cold Water Temperature Marsh Instrument Measures the temperature of the
12 Range: 0-60 oF, Increments: 1 oF
Gauge Company incoming cooling water.
Check for leaks and cracks.
Cooling Water Apparatus Cold Chicago Used to start flow of cooling water Always open when distillation
13
Valve Faucets into apparatus. column is in operation to supply
ample cold water.
Measures flow of cooling water into
Cold Water Rotameter Schutte & Check for leaks and cracks that
14 cooling coil.
(Measures in liquid GPM) Koerting Co. could cause malfunction
(Measures in liquid GPM)
Measures temperature of cooling
Check for any leaks or cracks that
15 Temperature Gauge Moeller water before entering cooling coil in
could cause malfunctions.
degrees Celsius.
Coil where heat transfer takes place
Check for any leaks or cracks that
16 Cooling Coil Na between distillate and cooling water
could cause malfunctions.
to provide total reflux.
17 Temperature Gauge Weksler Measures temperature of cooling Check for any leaks or cracks that
water exiting column in degrees could cause malfunctions.
Celsius.
Cold Chicago Allows cooling water to exit system Check for any leaks or cracks that
18 Cold Water Drain Valve
Faucets and drain. could spill water
Used to turn on heaters individually Check for any leaks or cracks that
19 Heat Controller Na
including heating jacket. could cause malfunctions.
Heat Supply for Heating Conducts electricity and passes it into Examine for loose wires or
20 Powerstat
Jacket the heating jacket malfunction
Check for loose wires or
Displays temperature taken at the
21 Digital Temperature Monitor Monogram malfunctions that may be
different thermocouples.
causedby leaks.
Measure temperature at different
stages in distillation column. Make sure probes are secure and
22 Thermocouples Omega
Reading outputs on Digital allow no leaks to touch them.
temperature display
Controls the electricity passing into Do not turn on unless cold water
Square D Safety
23 Power switch for heater the electric heating jacket turning it is flowing. Monitor temperatures
Switch
either on or off. and adjust as needed.
Heats the bottom of the distillation Very HOT. Exercise extreme
24 Electric Heating Jacket Na
column electrically. caution during operation.
Gas sample collected from the stage 2 sample Keep watch for leaks. Close when no
Gas Sample Collection Port
G2 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 2.
(collection port). ice. Clean up any spillage immedi
Gas sample collected from the stage 3 sample Keep watch for leaks. Close when no
Gas Sample Collection Port
G3 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 3.
(collection port). ice. Clean up any spillage immedi
Gas sample collected from the stage 4 sample Keep watch for leaks. Close when no
Gas Sample Collection Port
G4 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 4.
(collection port). ice. Clean up any spillage immedi
Gas sample collected from the stage5 sample Keep watch for leaks. Close when no
Gas Sample Collection Port
G5 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 5.
(collection port). ice. Clean up any spillage immedi
Gas sample collected from the stage 6 sample Keep watch for leaks. Close when no
Gas Sample Collection Port
G6 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 6.
(collection port). ice. Clean up any spillage immedi
Liquid sample collected from the stage 1 sample Keep watch for leaks. Close when no
Liquid Sample Collection Port
L1 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 1.
(collection port). ice. Clean up any spillage immedi
Liquid sample collected from the stage 2 sample Keep watch for leaks. Close when no
Liquid Sample Collection Port
L2 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 2.
(collection port). ice. Clean up any spillage immedi
Liquid sample collected from the stage 3 sample Keep watch for leaks. Close when no
Liquid Sample Collection Port
L3 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 3.
(collection port). ice. Clean up any spillage immedi
Liquid sample collected from the stage 4 sample Keep watch for leaks. Close when no
Liquid Sample Collection Port
L4 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 4.
(collection port). ice. Clean up any spillage immedi
Liquid sample collected from the stage5 sample Keep watch for leaks. Close when no
Liquid Sample Collection Port
L5 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 5.
(collection port). ice. Clean up any spillage immedi
Liquid sample collected from the stage 6 sample Keep watch for leaks. Close when no
Liquid Sample Collection Port
L6 Na plate via a sealed tube and release valve Keep samples cold by collecting sam
for stage 6.
(collection port). ice. Clean up any spillage immedi
5. Procedure
Distillation Column Operation:
1. Make a 5 mol% methanol solution by mixing it with water in the 13 gallon feed tank (4)
using graduated cylinders for measurement.
Note: make sure not to over fill the round bottom flask (7). It only needs to be filled
halfway or until the thermocouple (T1) is in contact with the mixture.
2. Pour the methanol-water mixture into the feed container and turn ON the three-way valve
in order to fill up the round bottom flask.
3. Open the cooling water supply valves (11 & 13) to supply cooling water to the distillation
column.
4. Start up the distillation column by turning on the power supply switches (22) to supply
heat to the distillation column.
5. Record the temperature of each of the thermocouples (T1-T9) located throughout the
column by analyzing the digital temperature monitor (21). Also record the readings of
the inlet cooling water temperature gauge (12), the outlet cooling water temperature
gauge (17), the inlet cooling water pressure gauge (15), and the cooling water rotameter
(14).
6. Make sure to collect the samples at each stage via the sample ports (G1-G6 &L1-
L6) of the distillation column and record the index of refraction by using the
Refractometer.
7. After the distillation process is done, make sure to turn OFF the heater power supply,
and the cooling water supply.
using a pipette.
2 Turn ON the Refractometer and the water heating system.
3 Open the prism assembly and remove the tissue.
4 Use a capillary tube to apply your liquid sample to the prism and close the prism
assembly.
NOTE: Be careful not to let the glass pipette tip touch the prism since this may scratch the
prism glass.
5 Adjust the toric lens, so the light shines on the prism and look through the eyepiece.
6 Analyze the index of refraction of the sample:
a When the index of refraction of your sample is close enough, then you will see
lighter region on the top and darker region on the bottom.
b If you cannot distinguish between these two regions then adjust the compensator
scale dial of the machine and the toric lens until the dark and light region is
completely separated.
Note: it is an iteration process between adjusting the light and the focus wheel located on the
front of the Refractometer.
c Once the clear distinguishable line between dark and light region is seen then
press the momentary contact switch located on the left hand side of the machine
until you see the scale. Then read off the index of refraction by looking at the
top scale and the refined bottom scale.
7 After you have noted down the index of refraction, record the temperature by
reading the temperature scale.
8 Make sure to clean the prism after testing each sample with a solvent and dabbing it with
tissue.
8. Error Analysis
Table 5: Sources of Uncertainty for Binary Distillation Lab
Component Manufacturer Uncertainty Expected Description
The 100mL graduated cylinder measures
100 mL Graduated Cylinder Nalgene 0.5mL liquid in increments of 1mL. The lines can
be accurately read to within 0.5mL
Via the manufactures website, the scale
Electronic Balance Denver Instrument Co. 0.01g used in this experiment has an associated
uncertainty of 0.01g
The temperature gauges measure in
Weksler
increments of 2 oF. By dividing the
Temperature Gauges & 1 oF
increments by 2 the expected uncertainty
Moeller
can be projected to be 1 oF.
The temperature monitor measures in
increments of 0.1 oC. The readings are
Digital Temperature Monitor Monogram 0.1 oC accurate when the column reaches steady
state and according to the manufacturers
website, are accurate to 0.1 oC.
The Refractometer measures the refractive
Refractometer index of a mixture in increments of 0.0002.
Bausch & Lomb 0.0001
However, the values can be read accurately
to the nearest 0.0001.
Listed above are components of the binary distillation lab whose specific uncertainties would
directly affect our recoded data. If these uncertainties were to occur, they would affect our
overall results by adding specific uncertainties to them.
9. References
1. Wankat, Phillip C.; Separation Process Engineering, second edition, Prentice Hall,
2007
3. Towler, G. and Sinnott, R., Chemical Engineering Design: Principles. BH, 2008
6. Edited by Don Green; John Perrys Chemical engineering Handbook, seventh edition,
McGraw-Hill, New York, 1997
7. Dean, John A., Lange's Handbook of Chemistry, 15th edition. New York, NY: John
Wiley & Sons, Inc., 1998.
9. Bennett C.O., Myers J.E., Momentum, Heat, and Mass transfer. 3 rd edition New York.
McGraw-Hill, 1982.